用气相色谱、气相色谱－质谱对萘普生重要中间体6－甲氧基－2－乙酰萘合成反应的研究

Study on Synthesis Reaction of 6-Methoxy-2-Acetonaphthalene──A Key Intermediate of Naproxen by Gas Chromatography(GC)and Gas Chromatography/Mass Spectrometry(GC/MS)

在优良抗风湿药物萘普生的重要中间体６－甲氧基－２－乙酰素的合成中存在溶剂硝基苯的毒性及所带来的污染。而改用二氯乙烷作溶剂，只加少量硝基苯即可。为配合合成工艺的优化，用气相色谱（ＧＣ）、气相色谱－质谱（ＧＣ／ＭＳ）对反应产物、副产物及多个杂质进行了定性分析研究，并在５％ＯＶ－１０１ＣｈｒｏｍｏｓｏｒｂＷＡＷＤＭＣＳ柱上完成了产物的内标定量分析。从而减少了副反应和高沸点杂质的生成，最终生产出了９５％以上含量的６－甲氧基－２－乙酰萘产品，收率达到６０％。

he 6-methoxy-2-acetonaphthalene was selectively obtained by direct acetylization of β-naphthalenemethyl ether promoted by AlCl_3 in the presence of nitrobenzene using 1,2-dichloroethane as solvent.The quantitative analysis of 6-methoxy-2-acetonaphthalene was performed by means of GC and the qualitativeanalysis for the intermediate and its isomers and by-products was carried out by GC and GC/MS.